CN110066402A - The preparation process of self-emulsification aqueous polyester emulsion - Google Patents
The preparation process of self-emulsification aqueous polyester emulsion Download PDFInfo
- Publication number
- CN110066402A CN110066402A CN201910357687.7A CN201910357687A CN110066402A CN 110066402 A CN110066402 A CN 110066402A CN 201910357687 A CN201910357687 A CN 201910357687A CN 110066402 A CN110066402 A CN 110066402A
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- Prior art keywords
- reaction kettle
- temperature
- self
- aqueous polyester
- preparation process
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses the preparation processes of self-emulsification aqueous polyester emulsion, are related to resin art, take raw material A-F by weight percentage, according to the sequence for launching powder dress solid material after first liquid delivery raw material, by in a part investment reaction kettle of A-E raw material, phosphite ester is finally put into, the batching hole on reaction kettle is closed, and use the air in nitrogen replacement reaction kettle, collet kettle heating agent is opened, material in reactor temperature reaches 150 DEG C, crawl stirring motor, after stirring no obstacle, stirring is opened.The present invention provides hydroxyl telechelic polyester, and using special hydrophilic monomer, polyester molecule segment itself has hydrophily, it is neutralized without amine, under low acid value state, water emulsification can be added, with water infinitely dissolve, co-solvent, to eliminate because after ammonia neutralization, waterborne polyester is easy hydrolysis and stores unstable problem, and the pollution problem of cosolvent, deposit that stability is good, the aqueous polyester resin of VOC free, to meet national standard and policy requirements.
Description
Technical field
The present invention relates to resin art, the preparation process of specially self-emulsification aqueous polyester emulsion.
Background technique
Traditional oiliness polyester resin, for solid content usually between 40~80%, remaining 60~20% is that volatility is molten
Agent, this high VOC resin, is used by many territorial restrictions, although emerging waterborne polyester can be solved partially, VOC is exceeded to be asked
Topic, but because using cosolvent problem, pollution is still difficult thoroughly to be solved, and domestic waterborne polyester is water after ammonia neutralization
Molten, storage stability is bad, and hydrolysis problem cannot solve always.
Summary of the invention
It is an object of the invention to: in order to solve the problems mentioned above in the background art, provide self-emulsification aqueous polyester
The preparation process of lotion.
To achieve the above object, the invention provides the following technical scheme: the preparation process of self-emulsification aqueous polyester emulsion, packet
Include the following steps:
Step 1: raw material A-F is taken by weight percentage；
Step 2: according to the sequence for launching powder dress solid material after first liquid delivery raw material, by a part of A-E raw material
It puts into reaction kettle, finally puts into phosphite ester；
Step 3: the batching hole on reaction kettle is closed, and uses the air in nitrogen replacement reaction kettle；
Step 4: collet kettle heating agent is opened；
Step 5: material in reactor temperature reaches 150 DEG C, and crawl stirring motor, after stirring no obstacle, unlatching is stirred
It mixes, adjusts and arrive process stipulation revolving speed；
Step 6: the temperature of charge in reaction kettle is increased to 180 DEG C from 150 DEG C；And it is kept the temperature；
Step 7: temperature increases 5 DEG C to reaction kettle per hour, until temperature reaches predetermined temperature, and increases nitrogen flow, makes
Reaction kettle is kept the temperature in predetermined temperature；
Step 8: sampling, and detection acid value is carried out, acid value reaches predetermined value for qualification；
Step 9: it is reduced to 80 DEG C F and to stir evenly hereinafter, being added the temperature of reaction kettle, is packed later.
Preferably, the phosphite ester in the step 2 is not directly thrown on the reaction kettle inner wall of heat.
Preferably, in the step 1 A-F be respectively 10~15% polyacid A, 25~32% binary acid B, 15~
20% hydrophily alcohol monomer C, 8~11.5% dihydric alcohol D, 0.1~0.5% catalyst E and 20~25% deionization
Water F.
Preferably, a length of 1h when heat preservation in the step 6.
Preferably, the predetermined temperature in the step 7 is 205 DEG C -215 DEG C, and a length of 2h when heat preservation in step 7.
Preferably, the acid value predetermined value in the step 8 is less than 8mgKOH/g.
Compared with prior art, the beneficial effects of the present invention are: the present invention provides hydroxyl telechelic polyester, using special hydrophilic
Monomer, polyester molecule segment itself have hydrophily, without amine neutralize, under low acid value state, water emulsification can be added, with water without
Limit is dissolved each other, co-solvent, to eliminate because after ammonia neutralization, waterborne polyester is easy hydrolysis and stores unstable problem, and helps
The pollution problem of solvent, deposits that stability is good, the aqueous polyester resin of VOC free, to meet national standard and policy requirements.
Detailed description of the invention
Fig. 1 is experimental data figure of the invention；
Fig. 2 is test result figure of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
It is mentioned in the present invention can market or it is private order obtained by.
The preparation process of self-emulsification aqueous polyester emulsion referring to FIG. 1-2, including the following steps:
Step 1: raw material A-F is taken by weight percentage；
Step 2: according to the sequence for launching powder dress solid material after first liquid delivery raw material, by a part of A-E raw material
It puts into reaction kettle, finally puts into phosphite ester；
Step 3: the batching hole on reaction kettle is closed, and uses the air in nitrogen replacement reaction kettle；
Step 4: collet kettle heating agent is opened；
Step 5: material in reactor temperature reaches 150 DEG C, and crawl stirring motor, after stirring no obstacle, unlatching is stirred
It mixes, adjusts and arrive process stipulation revolving speed；
Step 6: the temperature of charge in reaction kettle is increased to 180 DEG C from 150 DEG C；And it is kept the temperature；
Step 7: temperature increases 5 DEG C to reaction kettle per hour, until temperature reaches predetermined temperature, and increases nitrogen flow, makes
Reaction kettle is kept the temperature in predetermined temperature；
Step 8: sampling, and detection acid value is carried out, acid value reaches predetermined value for qualification；
Step 9: it is reduced to 80 DEG C F and to stir evenly hereinafter, being added the temperature of reaction kettle, is packed later.
Embodiment 1:
As the preferred embodiment of the present invention: the phosphite ester in step 2 not directly throws into the reaction kettle inner wall of heat
On, it avoids phosphite ester from being attached on reaction kettle inner wall, causes phosphite ester can not be to raw material A-F offer effect, phosphite ester
Belong to auxiliary antioxidant, play an important role in antioxidant systems, it is in addition to the energy with outstanding hydroperoxide decomposition
Power (this be hindered phenol primary antioxidant cannot), while there are also good color protective capabilities, it can be by hindered phenol antioxygen quilt
Dye radical drift after oxidation is shallow, in addition, it can also improve the processing temperature of polymer, has good cooperate with light stabilizer
Effect, and in calendering formation and extrusion molding with excellent fissility, roll banding and mold, do not improve throughput rate, inhibit
Wash rice goes out the generation of object.
Embodiment 2:
As the preferred embodiment of the present invention: in step 1 A-F be respectively 10~15% polyacid A, 25~32%
Binary acid B, 15~20% hydrophily alcohol monomer C, 8~11.5% dihydric alcohol D, 0.1~0.5% catalyst E and 20~
25% deionized water F, polyacid A are trimellitic anhydride, the trimellitic anhydride plasticizer excellent as heat resistance, weatherability
Raw material, and 10~15% polyacid A has the function of that surfactant, binary acid B are phthalic anhydride, exists as plasticising raw material,
The plasticity of mixed raw material is improved, dihydric alcohol is 1.4 butanediols, has good speedup and blast, by by A-F raw material
Hybrid process can effectively improve the performance of product.
Embodiment 3:
As the preferred embodiment of the present invention: a length of 1h when heat preservation in step 6 can make the material in reaction kettle abundant
It dissolves each other, at 180 DEG C of 1h, the raw material in reaction kettle can be made further to merge into each other, prevent the raw material in reaction kettle from polymerizeing
Phenomenon.
Embodiment 4:
As the preferred embodiment of the present invention: the predetermined temperature in step 7 is 205 DEG C -215 DEG C, and the guarantor in step 7
A length of 2h when warm after carrying out heat preservation fusion in step 6, carries out temperature raising and is kept the temperature again after temperature raising, up to 5h's
Promote the raw material in reaction kettle further mutually to merge during temperature raising, improves product quality, during prolonged heating,
Raw material in reaction kettle mutually blends, if temperature promotes the too fast pressure that will lead in reaction kettle and increases suddenly, will lead to peace
Full blast nearly increases.
Embodiment 5:
As the preferred embodiment of the present invention: the acid value predetermined value in step 8 is less than 8mgKOH/g, and acid value is fat
The mark of middle free fatty acid content, under conditions of fat production, acid value can be used as the index of hydrolysis degree, in its preservation
Under the conditions of, then it can be used as rancid index.Acid value is smaller, illustrates that oil quality is better, and freshness and refinement are better, and acid
Valence is determined by potentiometric titration.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
Claims (6)
1. the preparation process of self-emulsification aqueous polyester emulsion, it is characterised in that: include the following steps:
Step 1: raw material A-F is taken by weight percentage；
Step 2: according to the sequence for launching powder dress solid material after first liquid delivery raw material, a part of A-E raw material is put into
In reaction kettle, phosphite ester is finally put into；
Step 3: the batching hole on reaction kettle is closed, and uses the air in nitrogen replacement reaction kettle；
Step 4: collet kettle heating agent is opened；
Step 5: material in reactor temperature reaches 150 DEG C, and crawl stirring motor after stirring no obstacle, is opened stirring, adjusted
Save process stipulation revolving speed；
Step 6: the temperature of charge in reaction kettle is increased to 180 DEG C from 150 DEG C, and is kept the temperature；
Step 7: temperature increases 5 DEG C to reaction kettle per hour, until temperature reaches predetermined temperature, and increases nitrogen flow, makes to react
Kettle is kept the temperature in predetermined temperature；
Step 8: sampling, and detection acid value is carried out, acid value reaches predetermined value for qualification；
Step 9: it is reduced to 80 DEG C F and to stir evenly hereinafter, being added the temperature of reaction kettle, is packed later.
2. the preparation process of self-emulsification aqueous polyester emulsion according to claim 1, it is characterised in that: in the step 2
Phosphite ester not directly throw into heat reaction kettle inner wall on.
3. the preparation process of self-emulsification aqueous polyester emulsion according to claim 1, it is characterised in that: in the step 1
A-F be respectively 10~15% polyacid A, 25~32% binary acid B, 15~20% hydrophily alcohol monomer C, 8~
11.5% dihydric alcohol D, 0.1~0.5% catalyst E and 20~25% deionized water F.
4. the preparation process of self-emulsification aqueous polyester emulsion according to claim 1, it is characterised in that: in the step 6
Heat preservation when a length of 1h.
5. the preparation process of self-emulsification aqueous polyester emulsion according to claim 1, it is characterised in that: in the step 7
Predetermined temperature be 205 DEG C -215 DEG C, and a length of 2h when heat preservation in step 7.
6. the preparation process of self-emulsification aqueous polyester emulsion according to claim 1, it is characterised in that: in the step 8
Acid value predetermined value be less than 8mgKOH/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910357687.7A CN110066402A (en) | 2019-04-29 | 2019-04-29 | The preparation process of self-emulsification aqueous polyester emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910357687.7A CN110066402A (en) | 2019-04-29 | 2019-04-29 | The preparation process of self-emulsification aqueous polyester emulsion |
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| Publication Number | Publication Date |
|---|---|
| CN110066402A true CN110066402A (en) | 2019-07-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910357687.7A Pending CN110066402A (en) | 2019-04-29 | 2019-04-29 | The preparation process of self-emulsification aqueous polyester emulsion |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608456A (en) * | 2020-11-23 | 2021-04-06 | 江苏巨珩新材料科技有限公司 | Preparation process of pure water-based air-drying alkyd resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060069231A1 (en) * | 2002-10-22 | 2006-03-30 | Hiroshi Kajimaru | Aqueous polyester resin dispersion and method for production thereof |
| CN101824208A (en) * | 2010-04-09 | 2010-09-08 | 湖南大学 | Preparation method of aqueous polyester polyol dispersoid |
| CN105037698A (en) * | 2015-08-04 | 2015-11-11 | 江苏巨珩新材料科技有限公司 | Flowable solvent-free polyester resin and preparation technology and application thereof |
-
2019
- 2019-04-29 CN CN201910357687.7A patent/CN110066402A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060069231A1 (en) * | 2002-10-22 | 2006-03-30 | Hiroshi Kajimaru | Aqueous polyester resin dispersion and method for production thereof |
| CN101824208A (en) * | 2010-04-09 | 2010-09-08 | 湖南大学 | Preparation method of aqueous polyester polyol dispersoid |
| CN105037698A (en) * | 2015-08-04 | 2015-11-11 | 江苏巨珩新材料科技有限公司 | Flowable solvent-free polyester resin and preparation technology and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608456A (en) * | 2020-11-23 | 2021-04-06 | 江苏巨珩新材料科技有限公司 | Preparation process of pure water-based air-drying alkyd resin |
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Application publication date: 20190730 |
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